Reaktion #449588

Reaktionsgleichung

6,11-dihydro-5H-dibenz[b,e]azepine

4-[N-methyl-N-(2-methylbenzoyl)amino]benzoyl chloride

triethylamine

→

crystals

Ausbeute 78.1%

N-[4-[(6,11-Dihydro-5H-dibenz[b,e]azepin-5-yl)carbonyl]phenyl]-N-methyl-2-methylbenzamide

Ausbeute 78.1%

Lösungsmittel

tetrahydrofuran

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe solvent is removed
2. 2
   workup.ADDITIONthe residue diluted with water
3. 3
   Extraktionextracted with dichloromethane
4. 4
   WaschenThe extract is washed with 1N HCl water, 1M NaHCO3, brine
5. 5
   Trocknendried (Na2SO4)
6. 6
   EinengenThe filtrate is concentrated
7. 7
   Temperaturchilled

Vorschrift

A mixture of 0.291 g of 6,11-dihydro-5H-dibenz[b,e]azepine, 0.518 g of 4-[N-methyl-N-(2-methylbenzoyl)amino]benzoyl chloride and 0.182 g of triethylamine in 10 ml of tetrahydrofuran is stirred at room temperature for 2 hours. The solvent is removed, the residue diluted with water and extracted with dichloromethane. The extract is washed with 1N HCl water, 1M NaHCO3, brine and dried (Na2SO4). The solution is passed through a thin pad of hydrous magnesium silicate. The filtrate is concentrated and chilled to give 0.52 g of crystals, m.p. 160°-170° C.

Quelle